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“100 and More Basic NMR Experiments”
ISBN: 3-527-29091-5, VCH, Weinheim , 1996
- Chapter 1 : The NMR Spectrometer
1.1 Principles of an NMR Spectrometer 1.1.1 The Magnet
1.1.2 The Spectrometer Console 1.1.3 The Work-Station 1.1.4 Maintenance 1.2 Tuning a Probe-Head
1.2.1 Tuning and Matching with a Reflection Meter 1.2.2 Tuning and Matching with an R.F. Bridge and an Oscilloscope
1.2.3 Tuning and Matching with a Wobble Generator 1.3 The Lock Channel 1.4 The Art of Shimming 1.4.1 The Shim Gradients
1.4.2 The Shimming Procedure
- Chapter 2 Determination of the Pulse-Length
Exp. 2.1: Determination of the 90 1H Transmitter Pulse-Length
Exp. 2.2: Determination of the 90 13C Transmitter Pulse-Length Exp. 2.3: Determination of the 90 1H Decoupler Pulse-Length
Exp. 2.4: The 90 1H Pulse with Inverse Spectrometer Configuration Exp. 2.5: The 90 13C Decoupler Pulse with Inverse Configuration
Exp. 2.6: Determination of Radiofrequency Power
- Chapter 3 Routine NMR Spectroscopy and Standard Tests
Exp. 3.1: The Standard 1H NMR Experiment
Exp. 3.2: The Standard 13C NMR Experiment Exp. 3.3: Line-Shape Test for 1H NMR Spectroscopy
Exp. 3.4: Resolution Test for 1H NMR Spectroscopy Exp. 3.5: Sensitivity Test for 1H NMR Spectroscopy
Exp. 3.6: Line-Shape Test for 13C NMR Spectroscopy Exp. 3.7: ASTM Sensitivity Test for 13C NMR Spectroscopy
Exp. 3.8: Sensitivity Test for 13C NMR Spectroscopy Exp. 3.9: Quadrature Image Test
Exp. 3.10: Dynamic Range Test for Signal Amplitudes
- Chapter 4 Decoupling Techniques
Exp. 4.1: Decoupler Calibration for Homonuclear Decoupling
Exp. 4.2: Decoupler Calibration for Heteronuclear Decoupling Exp. 4.3: Low Power Calibration for Heteronuclear Decoupling
Exp. 4.4: Homonuclear Decoupling Exp. 4.5: The Homonuclear SPT Experiment
Exp. 4.6: The Heteronuclear SPT Experiment Exp. 4.7: 1D Nuclear Overhauser Difference Spectroscopy
Exp. 4.8: 1D NOE Spectroscopy with Multiple Selective Irradiation Exp. 4.9: 1H Off-Resonance Decoupled 13C NMR Spectra
Exp. 4.10: The Gated 1H-Decoupling Technique Exp. 4.11: The Inverse Gated 1H-Decoupling Technique
Exp. 4.12: 1H Single Frequency Decoupling of 13C NMR Spectra Exp. 4.13: 1H Low-Power Decoupling of 13C NMR Spectra
Exp. 4.14: Measurement of the Heteronuclear Overhauser Effect
- Chapter 5 Dynamic NMR Spectroscopy
Exp. 5.1: Low Temperature Calibration with Methanol
Exp. 5.2: High Temperature Calibration with 1,2-Ethanediol Exp. 5.3: Dynamic 1H NMR Spectroscopy on Dimethylformamide
Exp. 5.4: The Saturation Transfer Experiment
- Chapter 6 1D Multipulse Sequences
Exp. 6.1: Measurement of the Spin-Lattice Relaxation Time T1
Exp. 6.2: Measurement of the Spin-Spin Relaxation Time T2 Exp. 6.3: Editing 13C NMR Spectra with SEFT
Exp. 6.4: Editing 13C NMR Spectra with APT Exp. 6.5: The Basic INEPT Technique
Exp. 6.6: INEPT+Exp. 6.7: Refocused INEPT Exp. 6.8: Reverse INEPT
Exp. 6.9: Editing 13C NMR Spectra with DEPT Exp. 6.10: Editing 13C NMR Spectra with PENDANT
Exp. 6.11: 1D-INADEQUATE Exp. 6.12: The BIRD Filter Exp. 6.13: TANGO
Exp. 6.14: The Heteronuclear Double Quantum Filter Exp. 6.15: Water Suppression by Presaturation
Exp. 6.16: Water Suppression by the Jump and Return Method
- Chapter 7 NMR Spectroscopy with Selective Pulses
Exp. 7.1: Determination of a Shaped 90 1H Transmitter Pulse
Exp. 7.2: Determination of a Shaped 90 1H Decoupler Pulse Exp. 7.3: Determination of a Shaped 90 13C Decoupler Pulse
Exp. 7.4: Selective Excitation with DANTE Exp. 7.5: Selective COSY
Exp. 7.6: SELINCOR: Selective Inverse H,C Correlation via 1J(C,H) Exp. 7.7: SELINQUATE
Exp. 7.8: Selective TOCSY Exp. 7.9: INAPT
Exp. 7.10: Determination of Long Range C,H Coupling Constants Exp. 7.11: SELRESOLV Exp. 7.12: SERF
- Chapter 8 Auxiliary Reagents, Quantitative Determinations, and Reaction Mechanism
Exp. 8.1: Signal Separation Using a Lanthanide Shift Reagent
Exp. 8.2: Signal Separation of Enantiomers Using a Chiral Shift Reagent
Exp. 8.3: Signal Separation of Enantiomers Using a Chiral Solvating Agent
Exp. 8.4: Determination of Enantiomeric Purity with Pirkle's Reagent
Exp. 8.5: The Relaxation Reagent Cr(acac)3 Exp. 8.6: Quantitative 1H NMR Spectroscopy: Determination of the Alcohol Content of Polish
Vodka Exp. 8.7: Quantitative 13C NMR Spectroscopy with Inverse Gated1H-Decoupling
Exp. 8.8: Determination of Paramagnetic Susceptibility by NMR Exp. 8.9: The CIDNP Effect
- Chapter 9 Heteronuclear NMR Spectroscopy
Exp. 9.1: 1H-Decoupled 15N NMR Spectra with DEPT
Exp. 9.2: 1H-Coupled 15N NMR Spectra with DEPT Exp. 9.3: 19F NMR Spectroscopy
Exp. 9.4: 29Si NMR Spectroscopy with DEPT Exp. 9.5: 119Sn NMR Spectroscopy
Exp. 9.6: 2H NMR Spectroscopy Exp. 9.7: 11B NMR Spectroscopy
Exp. 9.8: 17O NMR Spectroscopy with RIDE
- Chapter 10 The Second Dimension
Exp. 10.1: 2D J-Resolved 1H NMR Spectroscopy
Exp. 10.2: 2D J-Resolved 13C NMR Spectroscopy Exp. 10.3: The Basic H,H-COSY Experiment
Exp. 10.4: Long-Range COSY Exp. 10.5: Phase-Sensitive COSY Exp. 10.6: Phase-Sensitive COSY-45
Exp. 10.7: Double Quantum Filtered COSY with Presaturation Exp. 10.8: C,H Correlation by Polarization Transfer (HETCOR)
Exp. 10.9: Long-Range C,H Correlation by Polarization Transfer Exp. 10.10: C,H Correlation via Long-Range Couplings (COLOC)
Exp. 10.11: The Basic HMQC Experiment Exp. 10.12: Phase-Sensitive HMQC with BIRD Selection and GARP Decoupling
Exp. 10.13: Phase-Sensitive HMBC with BIRD Selection Exp. 10.14: The Basic HSQC Experiment
Exp. 10.15: The HOHAHA or TOCSY Experiment Exp. 10.16: The NOESY Experiment Exp. 10.17: The CAMELSPIN or ROESY Experiment
Exp. 10.18: The HOESY Experiment Exp. 10.19: 2D-INADEQUATE Exp. 10.20: The EXSY Experiment
- Chapter 11 NMR Spectroscopy with Pulsed Field Gradients
Exp. 11.1: Calibration of Pulsed Field Gradients
Exp. 11.2: The Pulsed Gradient Spin-Echo Experiment Exp. 11.3: Gradient-Selected H,H-COSY
Exp. 11.4: Gradient-Selected Phase-Sensitive DQF COSY Exp. 11.5: Gradient-Selected HMQC
Exp. 11.6: Gradient-Selected HMBC Exp. 11.7: Phase-Sensitive Gradient-Selected HSQC
Exp. 11.8: Gradient-Selected TOCSY Exp. 11.9: Gradient-Selected HMQC-TOCSY
Exp. 11.10: Gradient-Selected 1H-Detected 2D INEPT-INADEQUATE Exp. 11.11: Gradient-Selected SELINCOR Exp. 11.12: GRECCO
Exp. 11.13: WATERGATE
- Chapter 12 The Third Dimension
Exp. 12.1: 3D HMQC-COSY
Exp. 12.2: 3D Gradient-Selected HSQC-TOCSY Exp. 12.3: 3D H,C,P-Correlation
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Known Bugs:
- page 3, line 4 from bottom: change "ms" into "microseconds"!
- page 56: Correct citation of Günthers Book in ref [1] see page 34, ref [4]
- page 155 second line: change to "p2, p4: 180 "
- page 158, line 8 from bottom: change "C-3" into "C-4"
- page 167, phase cycle for acquisition shoud read x, -x,-x, x, -x, x, x, -x
- page 173: change phase program for p2 to " -x, -x, x, x, -y, -y, y, y" and for aq to “ x,x, -x, -x, y, y, -y, -y"
- page 196: change in parameter list d2 to "1/[4J(C.,C)]"
- page 210: add in parameter list "p4: 90 13C decoupler pulse"
- page 237: In ref. [1] change publication year from "1958" into "1959"
- page 270: first line of pulse phases: change "p4" into "p5"
- page 272, line 4 from top: change "independent" into "dependent"
- page 289 and page 292: phase cycle for p2, change to x, -x, x, -x, y, -y, y, -y
- page 295: phase cycle for p4, change to y, -x, -y, x, -x, -y, x, y
- page 351, line 6 from top: change "have not diffused" into "have diffused"
- page 375, line 2 from top change "IH" into IH with superscript minus
- page 399: parameter list: d2: change 1/[2J(C,H) into 1/[4J(C,H)]
increment for t2 evolution: change 1/[2sw2] into 1/sw2
- page 403: change time requirements into 6h
add as second sentence: "Use appropriate pass and stop r.f. filters
in all three channels"
parameter list: d2: change 145 Hz into 160 Hz increment for t2
evolution 1/[2sw2] into 1/[4sw2]
add: "preacquisition delay as short as possible"
- page 406: 7th column, first row: add for Jeol instrument: "Alpha", "Lambda"
7th column, second row:add for Jeol Computer: "VAX Alpha AXP"
- page 407: parameter "pulse width": change the Jeol entry "Pwx" into "PWx"
parameter "delay": change the Jeol entry "Pix" into "PIx"
parameter "preacquisition delay": change the Varian entry "pad" into "rof2"
- page 408: second row of table: remove the Varian entries "ni"
Some of these errors have been corrected in the first reprint. Many thanks to all collegues who pointed our attention to these problems.
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